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Messages - Basquyatti

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1
Chemistry / The properties of GP nerve agent
« on: October 15, 2018, 10:58:03 pm »
GP, or 2,2-Dimethylcyclopentyl methylphosphonofluoridate, is a chiral, military grade toxicity organophosphorus compound, is a compound formulated in C8H16FO2P. GP forms a colorless and unscented liquid in pure form, in the impure form it is a colored liquid predominating several shades of amber by its degree of purity, with probable fruity smell coming from its closed chain alkoxy. GP has a boiling point of 222.49 degrees Celsius, being vacuum distilled, GP having more than double the vapor pressure of Ciclosarin, presented a vapor pressure of 0.094213 mmHg at 25 degrees Celsius, GP has an evaporation rate, evaporating 30 times slower than sarin, evaporating approximately 8 to 10 times slower than water.

GP is a persistent G-series persistent, similar to that of Ciclosarin, GP is extremely toxic, having high liposolubility by several means of exposure, especially percutaneously, GP is a nervous agent more toxic than Sarin and GH. GP is slightly soluble in water, persisting in it for days, it is speculated that it has a persistence higher than Ciclosarin and Soman in water due to its lower solubility, at high temperatures GP has a higher dissociation rate than GF. GP has high solubility in common organic solvents, as well as a good solubility rate in fats, oils, fatty acids, soap, lipids, triglycerides and the like. It has a persistence similar to that of Soman and Ciclosarin in environments, because it has a closed carbon chain and its persistence is considerably greater in any environment, but due to its greater evaporation than Ciclosarin, GP is thought to have lower persistence due to decomposition by air, GP as well as other G-series agent, is a non-persistent neurotoxic agent, exhibiting a low persistence in general, in normal environments, in normal environments and normal conditions, G-series agents are degraded within one week.

GP is disseminated by common means of dissemination, it is disseminated through common means, mines, chemical munitions, explosives, sprays, airplanes, sprayers, by missiles and rockets, pyrotechnic grenades, extinguishers, thermal grenades, propellants, cylinders, aerosols, nebulizers, humidifiers , polymer solutions (Lucite), piping tunnels, closed sites, closed complexes, atomizers and others, as well as other organophosphorous agents, GP is destroyed by bleach powder (alkaline components), satisfactory decontamination kits for G agents -series.

2
Chemistry / A new route of synthesis for G-series agents
« on: October 15, 2018, 06:12:57 am »
This process indicates and provides two direct steps for the manufacture of military-grade organophosphorus, such as G-series agents and the most unstable tammelin esters, following the equation, one mole of phosphoric acid is mixed in dichloromethane and reacted with a two mole of thionyl chloride with excess of a corresponding alkyl halide (isopropyl chloride, pinacolyl chloride, cyclohexyl chloride, such as other halides, iodide, bromide, fluoride has no efficacy and etc.) at the end of the emission of Hydrogen Chloride the Alkyl dichlorophosphate dissolved is directly reacted with 1 mol of Sodium Fluoride and a metal corresponding with methyl radical, at the end of the reaction the corresponding product obtained is directly distilled in vacuo and redistilled for the removal of the solvent.

3
GH is obtained similarly to Sarin using 3 steps, the first step is used for the manufacture of methylphosphonyl dichloride against Kinnear perren, an equimolar mixture between phosphorus trichloride, aluminum trichloride and chloromethane react to form a complex called APC, this is extracted and purified by conventional means, the second step consists of dissolving the APC in Dichloromethane and hydrolyzing it in hydrochloric acid in a molar ratio of 1 to 7, at the end of the reaction the lower phase is extracted and the DC separated from that solution, the DC is purified by common means, the third step is to react DC with sodium fluoride and 4-methylpentanol in molar ratio of 1: 1: 1, common means are used to dissolve the mixture and to promote At the end of the reaction the GH is extracted by common means.

https://fas.org/irp/threat/cbw/1951_CancellationofGHasadevelopmentprocurementtypeandrelatedaction.pdf

https://fas.org/irp/threat/cbw/1949_agentsoftheg-series.pdf

https://fas.org/irp/threat/cbw/1953_Significantaccomplishments_chemical%20corps.pdf

4
Chemistry / Synthesis conventional of Sarin
« on: October 02, 2018, 07:57:32 am »
Sarin is obtained in three steps, the first step is to produce methylphosphoryl dichloride (DC), DC is obtained by Kinnear-Perren reaction, which consists of using a mixture of one mole of phosphorus trichloride to be mixed with one mole of Aluminum trichloride at room temperature, then this mixture is placed in a freezer-filled vessel to react with an atmosphere of one mole of Chloromethane to give a mole of insoluble complex of ionic character with a melting point ranging from 275 degrees Celsius to 280 degrees Celsius, this complex is then filtered, weighed and dried to be dissolved in Dichloromethane and hydrolyzed in 36% hydrochloric acid, Hydrogen chloride serves to prevent the decomposition of DC, the reaction forms two phases in which are constituted by a higher acid water phase and a lower phase consisting of aluminum trichloride hexahydrated crystals, and a solution of DC and dichloromethane, the mixture is then separated by a separatory funnel, the insolubles filtered, the solvent distilled and the DC vacuum distilled to be purified, stored and prepared for the second step, the second step consists of dissolving a mole of DC in dichloromethane at room temperature and reacting with Hydrofluoric acid at low temperatures to form two phases, the upper phase is withdrawn and the lower one refluxed for the removal of the remaining hydrogen chloride, the material obtained is then brought to the third stage, where the DC obtained in the first step is added, adding Dichloromethane is used for the dissolution of more products and Isopropanol is added to the solution, the mixture is kept at room temperature (25 degrees Celsius) and then refluxed until all hydrogen chloride is emitted, the solvent is distilled and the Sarin distilled under vacuum. Note: Sarin and Dichloromethane may already be used for military stock or direct military operations, the mixture of Dichloromethane and Sarin tends to persist about 2X higher because the mixture is insoluble in water and not reactive in it.

Reaction GB (Di-Di, Hydrofluoric Acid)
 
Step 1. Preparation of methylphosphoryl Dichloride.

Using 138.72 grams of phosphorus trichloride 99%, place it in a pressure-suppressing apparatus and add 134.68 grams of anhydrous aluminum trichloride, stir the solution for 30 minutes at room temperature, after 30 minutes close the vessel, cool it to 0 degrees Celsius or below and introduce 51 grams of anhydrous Chloromethane, stir for 1 hour while introducing the agent and then let it react under pressure until there is no more in the vessel and the solution has completely crystallized, the end of the reaction is around 36 to 48 hours, filter the crystals and allow them to air dry or vacuum. Use 325 grams of crystals obtained from the first step to be placed in an open vessel, add 171.6 grams of Dichloromethane 99% into the vessel where the crystals are contained, begin stirring the mixture, stir the solution for 30 minutes and lower the temperature of the mixture to 0 degrees Celsius, after the time, add 305 ml of Hydrochloric Acid 36%, keeping the temperature at 0 degree Celsius and on vigorous agitation until it does not form more insoluble in the bottom of the container, see in times the formation of water and emission of Hydrogen Chloride, finished the formation of the upper phase with acidic water and there is no more the emission of Hydrogen Chloride, stop stir the mixture and bring the solution to a separatory funnel, stir the mixture a little to form the phase, leaving an exhaust outlet, forming the phases, remove the the lower phase where the DC is contained, then take the DC to filter and onwards, bring the mixture of DC and Dichloromethane to a Distillation Apparatus and distill Dichloromethane at 40 degrees Celsius and soon thereafter vacuum the DC of 75 degrees Celsius at 24 mmHg, the material obtained is a semi-solid mass at a temperature of 25 degrees Celsius. Stock the DC for the second step.

Step 2. Preparation of methylphosphoryl Difluoride (DF or Difluoro).

Take the DC product obtained from the first step and remove 67.81 grams from it and place in a vessel that is not attacked by Hydrofluoric Acid, shortly thereafter add 171.6 milliliters of Dichloromethane 99%, shake the mixture for 10 minutes and then then add 41.6875 grams of 48% hydrofluoric acid, cool the solution temperature to 0 degrees Celsius and start shaking it until no more hydrogen chloride is emitted, the emission is finished, stop shaking the solution, bring the solution to a separatory funnel, let two phases form in the solution and remove the product contained in the lower part, take the part removed and place it in a reflux apparatus and let reflux for the withdrawal of hydrogen chloride at cold reflux (-10 degree Celsius ) of 70 degrees Celsius. Finished the remaining emission of Hydrogen Chloride stops the reflux and leaves the material stocked in Teflon containers next to Dichloromethane until its use in the last step.

Step 3. Preparation of Sarin.

Take the material obtained, mixed with Dichloromethane and mix with the other 67.81 grams of DC and add 85.8 grams of Dichloromethane 99% therein, start shaking for 10 minutes at room temperature, add 60.1 milliliters of Isopropanol 99 , 98%, start shaking again for almost half an hour at room temperature, transfer the vessel to a cold (-10 degree Celsius) reflux apparatus, start stirring the mixture again and heat the solution to 75 degrees Celsius, stop heating until all hydrogen gas is emitted, or after 60 minutes. After the time has passed and there is no further emission of hydrogen chloride from the solution and there is no longer the formation of insolubles, stop the reflux, leave the solution temperature in the environment, filter the insolubles, distill the solvent at 40 degrees Celsius and then distill Sarin vacuum at 60 degree Celsius at 15 mmHg.


5
Chemistry / Re: Reaction CX-7 (Experimental)
« on: October 02, 2018, 12:12:33 am »
Yes, I am the Basquyati of the Portuguese Wikipedia

6
Chemistry / Re: The military preparation of FTH
« on: October 01, 2018, 10:15:39 pm »
Yes I read, the process is taken from the Preparatory Manual for Chemical Warfare

7
Chemistry / The military preparation of FTH
« on: October 01, 2018, 12:04:27 pm »
FTH is prepared from the dissolution of phosphoryl trichloride in solvent to react with dimethylamine at low temperatures to prevent boiling of the reactants, crystallizing the solution, sodium carbonate is added to dissolve the crystals and form dimethylaminophosphoryl chloride (Nitron-2B), the insolubles are filtered, the solvent distilled and the Nitron-2B distilled under vacuum, this material obtained is then dissolved in Chloroform and mixed with Ethanol and sodium fluoride and then this is refluxed at 65 degrees Celsius, the precipitated crystals are separated by addition of water for the dissolution of sodium chloride, the product phase is in the lower phase and is then extracted by separation funnel, the mixture is then placed to distill for the removal of chloroform, the crystals of FTH (FTHCl) are then dried outdoors or by vacuum filtration.

In a container add 156 grams of 98%~99% phosphoryl trichloride, then add 500 milliliters of anhydrous 1,2-Dichloroethene or Ethyl Ether, dissolve the agent at -5 degrees Celsius and when dissolved add 46 grams of 98% liquid Dimethylamine, shake the solution well and keep it below of -5 Celsius the reaction, then crystallization of the solution, when crystallization or crystallization is complete, add 107 grams of Sodium Carbonate 99% and leave the temperature to 0 degree Celsius and stir the solution during the reaction. precipitates from the first reaction will be dissolved and give room for a solid insoluble powder sodium bicarbonate when all the insolubles of the first reaction are dissolved, filter the solution, distill the solvent at 40~60 degrees Celsius the solvent and then distil at 90 degrees Celsius in 22 mmHg the Nitron-2B. In a flask place 163.58 grams of Dimethylaminophosphoryl dichloride and add 610 milliliters of chloroform 99%, dissolve it in it and thereafter add 46.53 grams of 99% Ethanol, keep the vessel under stirring before adding the Ethanol, add the Ethanol, add 42.5 grams of Sodium Fluoride 98%~99%, let the reaction take place on stirring in the reflux apparatus at 65 degrees Celsius, keep this reaction also on stirring, and more of two hours of reaction, a very simple method of knowing that the reaction is over is no longer the crystallization of Fluorotabun hydrochloride or Hydrochloride. The sodium chloride is dissolved in 170 milliliters of distilled water at 20 degrees Celsius, the solution is stirred for 5 minutes, then the water is filtered with the salt, the solvent is distilled at 65 degrees Celsius and the crystals are filtered through vacuum or let them air dry.

8
Chemistry / Reaction CX-7 (Experimental)
« on: September 15, 2018, 02:27:43 am »
My experimental synthesis to obtain Halogenated oximes.

Summary: This reaction uses a cheaper process of reducing Chloropicrin with the help of Magnesium and
anhydrous hydrogen chloride in a closed container, the standard solvent is Tetrahydrofuran, the reaction takes place at low temperatures and on vigorous shaking as soon as all the material is precipitated at the bottom, water is added to precipitate insoluble, then these are filtered, the solvent distilled and the CX purified by vacuum distillation.

Using 167.72 grams of PS 99%, place to mix with 600 grams of 99% THF at 0 degrees Celsius and place the mixture in a pressure-holding vessel, then introduce 49,102 grams of 99% Magnesium powder, and close the container with vigorously stir, pour into it 109.5 grams of anhydrous Hydrogen Chloride, the reaction ends when there is no more pressure in the vessel, then it filters the impurities, distills the solvent from 66 degrees Celsius up to 70 degrees Celsius and distils the agent at 58 degrees Celsius by 28 mmHg

Pages: [1]

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